Iodine → HCID 178485021, 화합물

HRID 543890노트

반응식

HRID 543890 반응식
[OH-].[Na+].Cl.[CH3:4][C:5]1[NH:9][CH:8]=[N:7][C:6]=1[CH2:10][SH:11].[C:12]([NH:14][C:15]([NH:20][CH3:21])=[N:16][CH2:17][CH2:18][SH:19])#[N:13].II>>[C:12]([NH:14][C:15]([NH:20][CH3:21])=[N:16][CH2:17][CH2:18][S:19][S:11][CH2:10][C:6]1[N:7]=[CH:8][NH:9][C:5]=1[CH3:4])#[N:13]

참가 물질

5

반응물 4

HCID 807Iodine2회HCID 14798Sodium HydroxideHCID 159163955-Methyl-4-mercaptomethylimidazole hydrochlorideHCID 178485018HCID 178485018, 화합물

생성물 1

HCID 178485021HCID 178485021, 화합물

실험 절차

Aqueous sodium hydroxide (3.60 g, 0.9 mol) was added to a stirred ethanolic solution of 5-methyl-4-mercaptomethylimidazole hydrochloride (5.92 g, 0.03 mol) and N-cyano-N'-methyl-N"-(2-mercaptoethyl)guanidine (5.74 g, 0.0363 mol). The solution was cooled to 0° and a saturated ethanolic solution of iodine was added until the iodine color remained. The solvent was removed under reduced pressure to yield an oil which was purified using preparative high pressure liquid chromatography (silica gel; 13% methanol in ethyl acetate). The glassy product obtained was triturated with acetonitrile to yield N-cyano-N'-methyl-N"-[2-(5-methyl-4-imidazolylmethyldithio)ethyl]guanidine, m.p. 137°-142°; MS m/e 284.

후처리

  1. temperatureThe solution was cooled to 0°
  2. customThe solvent was removed under reduced pressure
  3. customto yield an oil which
  4. customwas purified
  5. customThe glassy product obtained
  6. customwas triturated with acetonitrile

출처 및 근거

ORD 기록
ord-54062b7da6944e998e2f796dfc1923c8
출처 데이터셋
uspto-grants-1984_05
특허 번호
US04447621

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